CN111381440A - Photosensitive coverlay composition - Google Patents
Photosensitive coverlay composition Download PDFInfo
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- CN111381440A CN111381440A CN202010335397.5A CN202010335397A CN111381440A CN 111381440 A CN111381440 A CN 111381440A CN 202010335397 A CN202010335397 A CN 202010335397A CN 111381440 A CN111381440 A CN 111381440A
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- epoxy resin
- acrylate
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds
Abstract
The invention provides a photosensitive covering film composition. The photosensitive covering film composition comprises, by weight, 100 parts of alkali-soluble epoxy acrylic resin, 1-40 parts of epoxy resin, 1-40 parts of acrylate monomers, 0.1-10 parts of photoinitiators, 10-40 parts of rutile titanium dioxide and 0.5-2 parts of auxiliaries. The photosensitive covering film composition can effectively improve the reflectivity of the product by introducing rutile titanium dioxide, and can realize continuous coating and has good thickness uniformity by matching with other components and dosage proportions. Meanwhile, the composition can be developed in an alkaline solution and is negatively imaged, has good flexibility after curing and has excellent heat resistance. In a word, the photosensitive covering film composition has the advantages of uniform film formation, few surface defects, short film formation process, high whiteness and reflectivity, good flexibility, high temperature resistance and the like, and can completely replace the traditional white ink to be applied to the LED lamp strip.
Description
Technical Field
The invention relates to the technical field of printed circuit boards, in particular to a photosensitive covering film composition.
Background
With the development of information communication technology, the high-speed development of the microelectronic field is driven, and the printed circuit board is widely applied to multiple fields such as mobile phones, computers, display screens and the like. The printed circuit board mainly comprises a soft board printed circuit, a hard board printed circuit and a soft and hard combined board printed circuit, the traditional printed circuit board usually adopts solder resist ink which can protect the circuit board from being eroded by dust, moisture and chemicals, but the solder resist ink is not resistant to folding and cannot be used in the soft board and the soft and hard combined board, so that the photosensitive cover film is produced. The photosensitive cover film is used as a substitute for photosensitive ink and the cover film, has double advantages, can meet the requirements of manufacturing printed circuits of soft boards and hard boards, can be applied to soft and hard combination boards, and is wider in application.
Because the LED lamp belt has the three characteristics of energy conservation, environmental protection, long service life and the like, the application field of the LED lamp belt is continuously expanded, the types and the quantity of application products are continuously increased, the investment on the LED industry in the current market is continuously increased, and the demand is more and more vigorous. However, at present, white ink is mostly used for preparing the LED strip for increasing the light emitting effect of the product, and there are many disadvantages, firstly, in the process of using the screen printing, the white ink has uneven thickness and many surface defects, which affect the product quality; secondly, the white ink needs to be baked for two times at low temperature, so that the working procedure is increased, the working hours are consumed, and the folding resistance, the flexibility resistance, the weather resistance and other properties of the ink are greatly insufficient, so that the expansion application of the LED lamp strip is limited to a certain extent.
Therefore, there is a need to develop a white photosensitive covering film composition with high reflectivity to better replace white ink for application in a lamp strip.
Disclosure of Invention
The invention mainly aims to provide a photosensitive covering film composition which has uniform film thickness and few surface defects, has better whiteness and higher reflectivity, and has good flexibility and high temperature resistance after being coated on an insulating base film, so that the photosensitive covering film composition can be better used for replacing white ink to be applied to an LED lamp strip.
In order to achieve the above object, according to one aspect of the present invention, there is provided a photosensitive cover film composition comprising 100 parts by weight of an alkali-soluble epoxy acrylic resin, 1 to 40 parts by weight of an epoxy resin, 1 to 40 parts by weight of an acrylate monomer, 0.1 to 10 parts by weight of a photoinitiator, 10 to 40 parts by weight of rutile titanium dioxide, and 0.5 to 2 parts by weight of an auxiliary agent.
Further, the weight part of the titanium dioxide is 10-20 parts; preferably, the rutile type titanium dioxide is one or more of R907, R900, R920, R931, R960, R102, R103, R104 and R105.
Further, the acid value of the alkali-soluble epoxy acrylic resin is 60-150 mg KOH/g, preferably 80-120 mg KOH/g.
Further, the alkali-soluble epoxy acrylic resin is one or more of carboxylic acid modified bisphenol A epoxy resin, carboxylic acid modified bisphenol F epoxy resin and carboxylic acid modified novolac epoxy resin.
Further, the epoxy resin has an epoxy equivalent of 160 to 500g/eq and contains at least two epoxy groups; preferably, the epoxy resin is one or more of bisphenol epoxy resin, biphenyl epoxy resin, novolac epoxy resin, epoxy resin containing naphthalene ring and alicyclic epoxy resin; more preferably, the epoxy resin is a bisphenol type epoxy resin.
Further, the weight part of the epoxy resin is 10-30 parts.
Further, the acrylate monomer is one or more of monofunctional group (methyl) acrylate, difunctional group (methyl) acrylate, trifunctional group (methyl) acrylate and multifunctional group (methyl) acrylate; preferably, the monofunctional (meth) acrylate is one or more of (ethoxy) phenol (meth) acrylate, stearic acid acrylate, ethoxy (propoxy) nonylphenol (meth) acrylate, ethoxy (propoxy) tetrahydrofurfuryl (meth) acrylate; preferably, the difunctional (meth) acrylate is one or more of 1, 6-hexanediol diacrylate, tricyclodecanedimethanol diacrylate, dioxane glycol diacrylate, ethoxylated (propoxylated) bisphenol a di (meth) acrylate, polyethylene glycol (400) diacrylate, polypropylene glycol (600) diacrylate; preferably, the trifunctional (meth) acrylate is one or more of ethoxy (propoxy) trimethylolpropane tri (meth) acrylate, pentaerythritol triacrylate, tris (2-hydroxyethyl) isocyanurate triacrylate; preferably, the multifunctional (meth) acrylate is one or more of dipentaerythritol hexaacrylate, ethoxylated pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate.
Further, the weight average molecular weight of the acrylate monomer is 200-1000, and the glass transition temperature is-30-60 ℃; preferably, the weight part of the acrylate monomer is 5-30 parts.
Further, the photoinitiator comprises a photopolymerization initiator and a photosensitizer, and the weight ratio of the photopolymerization initiator to the photosensitizer is preferably (150-200): 1.
Further, the photopolymerization initiator is one or more selected from 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 1- [4- (2-hydroxy) -phenyl ] -3-hydroxy-2-methyl-1-propanone-1-one, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, bis (2,4, 6-trimethylbenzoyl) phenylphosphine oxide, ethyl 2,4, 6-trimethylbenzoyl phenylphosphinate, 2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone, and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone Seed growing; preferably, the photosensitizer is one or more of 2, 4-diethyl oxalate, 2-isopropyl thioxanthone, 2, 4-diethyl thioxanthone and benzophenone.
Further, the weight part of the photoinitiator is 1-5 parts.
Further, the auxiliary agent comprises one or more of a flatting agent, a defoaming agent, a dispersing agent and an adhesion promoter; preferably, the leveling agent is one or more of BYK333, BYK358, BYK306, BYK394 and BYK322, the defoaming agent is one or more of BYK066N, BYK175, BYK015 and BYK1730, the dispersing agent is one or more of BKY110, BYK111 and BYK9077, and the adhesion promoter is BYK 4510.
Further, the weight part of the auxiliary agent is 1-1.5 parts.
The photosensitive covering film composition comprises, by weight, 100 parts of alkali-soluble epoxy acrylic resin, 1-40 parts of epoxy resin, 1-40 parts of acrylate monomers, 0.1-10 parts of a photoinitiator, 1-40 parts of rutile titanium dioxide and 0.5-2 parts of an auxiliary agent. The photosensitive covering film composition can effectively improve the reflectivity of the product by introducing rutile titanium dioxide, and can realize continuous coating and good thickness uniformity by matching with other components and dosage proportions. Meanwhile, the composition can be developed in an alkaline solution and can be subjected to negative-working imaging (short process), has good flexibility after curing and has excellent heat resistance. In a word, the high-reflection white photosensitive covering film composition provided by the invention has the advantages of uniform film formation, few surface defects, short film formation process, high whiteness and reflectivity, good flexibility, high temperature resistance and the like, and can completely replace the traditional white ink to be applied to the LED lamp strip. Compared with solder resist ink, the white photosensitive covering film provided by the invention adopts a single-component form, and can achieve the beneficial effects of good film forming property, high temperature resistance, flexibility, whiteness, light reflectivity and the like on the basis that the content of rutile titanium dioxide (the proportion of the rutile titanium dioxide to alkali-soluble epoxy acrylic resin is less than or equal to 40%) is far lower than the content of the titanium dioxide in the solder resist ink.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As described in the background section of the present invention, the use of white ink to prepare LED strips for increasing the light emitting effect of the product has many disadvantages, such as uneven ink thickness, many surface defects, long film forming process, insufficient refractive index, and insufficient folding resistance, flexing resistance, and heat resistance, which limits the LED strips from being expanded to some extent.
In order to solve the problems, the invention provides a photosensitive covering film composition which comprises, by weight, 100 parts of alkali-soluble epoxy acrylic resin, 1-40 parts of epoxy resin, 1-40 parts of acrylate monomers, 0.1-10 parts of a photoinitiator, 10-40 parts of rutile titanium dioxide and 0.5-2 parts of an auxiliary agent.
The photosensitive covering film composition can effectively improve the reflectivity of the product by introducing rutile titanium dioxide, and can realize continuous coating and good thickness uniformity by matching with other components and dosage proportions. Meanwhile, the composition can be developed in an alkaline solution and is negatively imaged, has good flexibility after curing and has excellent heat resistance. In a word, the high-reflection white photosensitive covering film composition provided by the invention has the advantages of uniform film formation, few surface defects, short film formation process (continuous coating and rapid curing can be realized), high whiteness and reflectivity, good flexibility, high temperature resistance and the like, and can completely replace the traditional white ink to be applied to the LED lamp strip.
For rutile titanium dioxide, compared with other white inorganic fillers such as talc, barium sulfate, white mill base, etc., rutile titanium dioxide has many advantages, such as: (1) the refractive index is higher; (2) the decoloring force is better; (3) the covering power is better; (4) the oil absorption is better. Therefore, the rutile titanium dioxide is introduced into the white photosensitive covering film composition, and the beneficial effects can be achieved by matching with the selection and the dosage relation of other components.
In order to improve the wettability, the dispersibility and the coating property of the titanium dioxide, in a preferred embodiment, the auxiliary agent comprises one or more of a leveling agent, a defoaming agent, a dispersing agent and an adhesion promoter. Thus, based on the introduction of rutile titanium dioxide with specific content and the selection of the auxiliary agents, the performance of the photosensitive covering film composition can be further improved, and the negative photosensitive covering film with high heat resistance, low modulus and low warpage can be formed more favorably. The leveling agent is one or more of BYK333, BYK358, BYK306, BYK394 and BYK322, the defoaming agent is one or more of BYK066N, BYK175, BYK015 and BYK1730, the dispersing agent is one or more of BKY110, BYK111 and BYK9077, and the adhesion promoter is BYK4510 and the like. More preferably, the weight part of the auxiliary agent is 1-1.5 parts.
In a preferred embodiment, the weight part of the rutile type titanium dioxide is 10-20 parts. Controlling the weight portion of the rutile titanium dioxide within the range is more favorable for improving the whiteness and the reflectivity of the photosensitive covering film composition, and can also consider other aspects such as film forming property, flexibility, high temperature resistance and the like. Preferably, titanium dioxide includes, but is not limited to, one or more of R907, R900, R920, R931, R960, R102, R103, R104, R105.
In a preferred embodiment, the acid value of the alkali-soluble epoxy acrylic resin is 60 to 150mg KOH/g, preferably 80 to 120mg KOH/g, and the acid value in the range is good for resin exposure developing performance, and improves compatibility with other components, and improves film forming property, curing property and the like.
In a preferred embodiment, the epoxy resin has an epoxy equivalent of 160 to 500g/eq and contains at least two epoxy groups, from the viewpoint of soldering heat resistance, developability, and adhesion; preferably, the epoxy resin includes, but is not limited to, one or more of bisphenol type epoxy resin (including bisphenol a type, bisphenol F type, bisphenol S type, etc.), biphenyl type epoxy resin, novolac epoxy resin (including phenol novolac type, etc.), epoxy resin containing naphthalene ring, alicyclic epoxy resin; more preferably, the epoxy resin is a bisphenol type epoxy resin. More preferably, the epoxy resin is 10 to 30 parts by weight. By controlling the weight part of the epoxy resin within the above range, the film-forming property of the composition and the heat resistance after curing can be further improved.
In a preferred embodiment, the acrylate monomers include, but are not limited to, one or more of monofunctional (meth) acrylates, difunctional (meth) acrylates, trifunctional (meth) acrylates, and multifunctional (meth) acrylates. It should be noted that the above-mentioned "polyfunctional" means that the number of functional groups is more than 3. The acrylate monomers have excellent comprehensive performance and are more suitable for being applied to the photosensitive covering film composition. Preferably, the monofunctional (meth) acrylate includes, but is not limited to, one or more of (ethoxy) phenol (meth) acrylate, stearic acid acrylate, ethoxy (propoxy) nonylphenol (meth) acrylate, ethoxy (propoxy) tetrahydrofurfuryl (meth) acrylate; preferably, difunctional (meth) acrylates include, but are not limited to, one or more of 1, 6-hexanediol diacrylate, tricyclodecane dimethanol diacrylate, dioxane diol diacrylate, ethoxylated (propoxylated) bisphenol a di (meth) acrylate, polyethylene glycol (400) diacrylate, polypropylene glycol (600) diacrylate; preferably, the trifunctional (meth) acrylate includes, but is not limited to, one or more of ethoxy (propoxy) trimethylolpropane tri (meth) acrylate, pentaerythritol triacrylate, tris (2-hydroxyethyl) isocyanurate triacrylate; preferably, the multifunctional (meth) acrylate includes, but is not limited to, one or more of dipentaerythritol hexaacrylate, ethoxylated pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate.
More preferably, the weight average molecular weight of the acrylate monomer is 200-1000, and the glass transition temperature is-30-60 ℃. Thus being more beneficial to improving the film forming property of the composition and the high temperature resistance of the thick film. More preferably, the weight part of the acrylate monomer is 5 to 30 parts.
In a preferred embodiment, the photoinitiator comprises a photopolymerization initiator and a photosensitizer, and the weight ratio of the photopolymerization initiator to the photosensitizer is preferably (150-200): 1. In order to improve the reflectance and avoid the problems of insufficient curing degree and yellowing resistance caused by adding rutile titanium dioxide to the photosensitive covering film, the photopolymerization initiator is preferably 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 1- [4- (2-hydroxy) -phenyl ] -3-hydroxy-2-methyl-1-propanon-1-one, 2,4, 6-trimethylbenzoyl-diphenyl phosphorus oxide, bis (2,4, 6-trimethylbenzoyl) phenyl phosphine oxide, ethyl 2,4, 6-trimethylbenzoyl phenyl phosphonate, 2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-one -one or more of acetone, 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone; preferably, the photosensitizer is one or more of 2, 4-diethyl oxalate, 2-isopropyl thioxanthone, 2, 4-diethyl thioxanthone and benzophenone. Particularly, an initiation system formed by matching 2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-acetone and/or 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone with the photosensitizer can achieve higher reflectivity by using a small amount of titanium dioxide, and has more obvious effects on improving the properties of the adhesive force, yellowing resistance and the like of the covering film. Moreover, the initiation system is matched with the auxiliary agent, so that the performances such as the adhesive force of the covering film, yellowing resistance and the like are further promoted, and the photosensitive covering film provided by the invention has more outstanding comprehensive performances.
For the purpose of improving curing efficiency while reducing resource consumption, in a preferred embodiment, the photoinitiator is present in an amount of 1 to 5 parts by weight.
The preparation method of the photosensitive coverlay composition provided by the invention can adopt a method commonly used in the field, and in order to mix and disperse the components more fully, in a preferred embodiment, the preparation process is as follows:
the components of the photosensitive covering film composition are weighed in proportion and placed in a beaker, uniformly stirred under the high-speed stirring of a high-speed dispersion stirrer, the rotating speed is preferably 1000-3000 r/min, the stirring is carried out for at least 2 hours, and the processes of film coating, film pasting, exposure, development, curing and the like are carried out. The method comprises the following specific steps: firstly, coating a film by a wire rod method, prebaking at 80 ℃ for 15-30 min, carrying out hot roller film pasting after prebaking is finished, and then exposing (energy is 100-300 mJ.cm)-2) And then developed (1.0 wt% Na as a developer solution)2CO3The developing time of the solution is 60-90 s, the developing temperature is 29 +/-1 ℃, the spraying pressure is 0.2-0.4 MPa, and finally the developed sample is subjected to thermosetting treatment (150-200 ℃ and 1 h).
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added 2.0g of an acrylic monomer (of which 0.5g of ethoxybisphenol A diacrylate, 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.603g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone)), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 5g of rutile type titanium dioxide (R907), 6.0g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin, 3.0g of a toughening epoxy resin), 0.1g of defoaming agent BYK066N, 0.2g of dispersing agent BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510 are stirred at a high speed, dissolved and dispersed, and finally filtered to prepare varnish which is stored in dark light for later use.
Example 2
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added 2.0g of acrylic monomers (of which 0.5g of ethoxybisphenol A diacrylate and 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.603g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 5g of titanium dioxide (R960), 6.0g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin and 3.0g of a toughening epoxy resin), 0.1g of a defoaming agent BYK066N, 0.2g of dispersant BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510, stirring at high speed for dissolving and dispersing, finally filtering to prepare varnish, and storing in dark for later use.
Example 3
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added 2.0g of acrylic monomers (of which 0.5g of ethoxybisphenol A diacrylate and 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.603g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 5g of titanium dioxide (R105), 6.0g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin and 3.0g of a toughening epoxy resin), 0.1g of a defoaming agent BYK066N, 0.2g of dispersant BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510, stirring at high speed for dissolving and dispersing, finally filtering to prepare varnish, and storing in dark for later use.
Example 4
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added 2.0g of acrylic monomers (of which 0.5g of ethoxybisphenol A diacrylate and 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.603g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 3g of titanium dioxide (R960), 6.0g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin and 3.0g of a toughening epoxy resin), 0.1g of a defoaming agent BYK066N, 0.2g of dispersant BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510, stirring at high speed for dissolving and dispersing, finally filtering to prepare varnish, and storing in dark for later use.
Example 5
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added 2.0g of acrylic monomers (of which 0.5g of ethoxybisphenol A diacrylate and 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.603g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 4g of titanium dioxide (R960), 6.0g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin and 3.0g of a toughening epoxy resin), 0.1g of a defoaming agent BYK066N, 0.2g of dispersant BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510, stirring at high speed for dissolving and dispersing, finally filtering to prepare varnish, and storing in dark for later use.
Example 6
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added 2.0g of an acrylic monomer (of which 0.5g of ethoxybisphenol A diacrylate and 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.603g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 4g of rutile titanium dioxide (R907), 6.0g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin and 3.0g of a toughened epoxy resin), 0.1g of a defoaming agent BYK066N, 0.2g of dispersant BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510, stirring at high speed for dissolving and dispersing, finally filtering to prepare varnish, and storing in dark for later use.
Example 7
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 80mg KOH/g) were added 2.8g of an acrylic monomer (of which 0.5g of ethoxybisphenol A diacrylate, 2.2g of 30 ethoxybisphenol A dimethacrylate), 0.603g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone)), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 8g of rutile type titanium dioxide (R907), 8g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin, 3.0g of a toughening epoxy resin), 0.1g of defoaming agent BYK066N, 0.2g of dispersing agent BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510 are stirred at a high speed, dissolved and dispersed, and finally filtered to prepare varnish which is stored in dark light for later use.
Example 8
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 120mg KOH/g) were added 8g of an acrylic monomer (of which 0.5g of ethoxybisphenol A diacrylate and 13.2g of 30 ethoxybisphenol A dimethacrylate), 3g of a photopolymerization initiator (of which 1g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone)), 1.5g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.5g of a photosensitizer ITX (2-isopropylthioxanthone)), 2g of rutile type titanium dioxide (R907), 0.2g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin and 3.0g of a toughening epoxy resin), 0.1g of defoaming agent BYK066N, 0.2g of dispersing agent BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510 are stirred at a high speed, dissolved and dispersed, and finally filtered to prepare varnish which is stored in dark light for later use.
Example 9
Preparation of high-reflectance white photosensitive coverlay composition: 100g of alkali-soluble photosensitive epoxy acrylic resin (acid value 80mg KOH/g) were added 1g of acrylic monomer (0.5 g of ethoxylated bisphenol A diacrylate, 0.5g of 30 ethoxylated bisphenol A dimethacrylate), 3g of photopolymerization initiator (1.5 g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone)), 1.5g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.0015g of photosensitizer ITX (2-isopropylthioxanthone)), 10g of rutile titanium dioxide (R907), 1g of epoxy resin (3.0 g of bisphenol A epoxy resin, 3.0g of toughening epoxy resin), 0.4g of defoaming agent BYK066N, 0.8g of dispersing agent BYK110, 0.4g of flatting agent BYK333 and 0.4g of adhesion promoter BYK4510 are stirred at a high speed, dissolved and dispersed, and finally filtered to prepare varnish which is stored in dark light for later use.
Example 10
Preparation of high-reflectance white photosensitive coverlay composition: to 100g of an alkali-soluble photosensitive epoxy acrylic resin (acid value: 80mg KOH/g), 16.8g of an acrylic monomer (of which 3.6g of ethoxybisphenol A diacrylate, 13.2g of 30 ethoxybisphenol A dimethacrylate), 6.03g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone)), 3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.03g of a photosensitizer ITX (2-isopropylthioxanthone)), 40g of rutile type titanium dioxide (R907), 30g of an epoxy resin (of which 15g of bisphenol A epoxy resin, 15g of a toughening epoxy resin), 0.5g of defoaming agent BYK066N, 0.5g of dispersing agent BYK110, 0.5g of flatting agent BYK333 and 0.5g of adhesion promoter BYK4510 are stirred at a high speed, dissolved and dispersed, and finally filtered to prepare varnish which is stored in dark light for later use.
Example 11
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added successively 2.0g of an acrylic monomer (of which 0.5g of ethoxybisphenol A diacrylate, 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.6g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone)), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 5g of rutile type titanium dioxide (R960), 6.0g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin, 3.0g of a toughening epoxy resin), 0.1g of defoaming agent BYK066N, 0.2g of dispersing agent BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510 are stirred at a high speed, dissolved and dispersed, and finally filtered to prepare varnish which is stored in dark light for later use.
Example 12
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added 2.0g of an acrylic monomer (of which 0.5g of ethoxybisphenol A diacrylate, 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.6g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone)), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 5g of rutile type titanium dioxide (R900), 6.0g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin, 3.0g of a toughening epoxy resin), 0.1g of defoaming agent BYK066N, 0.2g of dispersing agent BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510 are stirred at a high speed, dissolved and dispersed, and finally filtered to prepare varnish which is stored in dark light for later use.
Comparative example 1
Preparation of high-reflectance white photosensitive coverlay composition: 20g of alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added with 2.0g of acrylic monomer (0.5 g of ethoxybisphenol A diacrylate and 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.6g of photopolymerization initiator (0.3 g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of photosensitizer ITX (2-isopropylthioxanthone)), 2g of titanium dioxide (R902, anatase titanium dioxide), 6.0g of epoxy resin (3.0 g of bisphenol A epoxy resin and 3.0g of toughening epoxy resin), 0.1g of defoaming agent BYK066N, 0.1g of dispersing agent BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510 are stirred at a high speed, dissolved and dispersed, and finally filtered to prepare varnish which is stored in dark light for later use.
Comparative example 2
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added 2.0g of acrylic monomers (of which 0.5g of ethoxybisphenol A diacrylate and 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.6g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 10g of titanium dioxide (R960), 6.0g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin and 3.0g of a toughening epoxy resin), 0.1g of a defoaming agent BYK066N, 0.2g of dispersant BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510, stirring at high speed for dissolving and dispersing, finally filtering to prepare varnish, and storing in dark for later use.
Comparative example 3
Preparation of high-reflectance white photosensitive coverlay composition: 20g of an alkali-soluble photosensitive epoxy acrylic resin (acid value 100mg KOH/g) were added 2.0g of an acrylic monomer (of which 0.5g of ethoxybisphenol A diacrylate and 1.5g of 30 ethoxybisphenol A dimethacrylate), 0.6g of a photopolymerization initiator (of which 0.3g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of a photosensitizer ITX (2-isopropylthioxanthone)), 2g of talc, 6.0g of an epoxy resin (of which 3.0g of bisphenol A epoxy resin and 3.0g of a toughening epoxy resin), 0.1g of a defoaming agent BYK06 066N, 0.2g of a dispersant BYK110, 0.1g of flatting agent BYK333 and 0.1g of adhesion promoter BYK4510, stirring at a high speed for dissolving and dispersing, finally filtering to prepare varnish, and storing in dark for later use.
Comparative example 4
Preparation of high reflectance two-component solder resist ink composition: the component A is prepared by adding 2.0g of acrylic monomers (0.5 g of ethoxy bisphenol A diacrylate and 1.5g of 30g of ethoxy bisphenol A dimethacrylate) into 20g of alkali-soluble photosensitive epoxy acrylic resin (the acid value is 100mg KOH/g), 0.6g of photopolymerization initiator (0.3 g of 2959 (2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone)), 0.3g of 907 (2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone)), 0.003g of photosensitizer ITX (2-isopropyl thioxanthone)), 10g of rutile type titanium dioxide (R900), 0.1g of defoamer BYK066N, 0.2g of dispersant BYK110, 0.1g of flatting agent BYK333, 0.1g of adhesion promoter BYK4510, the component B is 6.0g of epoxy resin (3.0 g of bisphenol A epoxy resin and 3.0g of toughening epoxy resin), 5g of rutile titanium dioxide (R900), 6.0g of acrylic acid monomer and 5g of solvent, and is stirred at a high speed, dissolved and dispersed, and finally filtered to prepare varnish, and the varnish is stored in dark for later use. When in use, the ratio of A: b3: 1 mixed and used over 24 hours, otherwise the exposure developed cured.
The obtained photosensitive epoxy acrylic resin varnish coating films of examples 1 to 12 and comparative examples 1 to 4 were evaluated as follows:
1. cured film bending resistance test
The evaluation was made in accordance with JIS-C-5-016 standard 8.7 and on the following criteria.
◎, no crack on the cured film.
○, cracks were found in the cured film.
× cracks in the cured film
2. Comparison of soldering Heat resistance
See IPC-TM650.2.6.8 standard. The cured film was vertically immersed in a tin furnace at a temperature of 300 ℃ for 30 seconds, and the surface was observed for blistering, discoloration, lifting, peeling, and the like, and the change in appearance was evaluated on the basis described below.
◎ no change in appearance
○ color change on the surface of the cured film
× the solidified film has floating, thin and deep soldering
3. Comparison of acid and alkali resistance
The prepared photosensitive cover film was immersed in 10% by mass hydrochloric acid and 10% by mass aqueous sodium hydroxide solution for 30min, and the surface was observed for blistering, discoloration, floating, peeling, and the like, and the change in appearance was evaluated on the following basis.
◎ no change in appearance
○ color change on the surface of the cured film
× the solidified film has floating, thin and deep soldering
4. Comparison of reflectance
And (4) testing the reflectivity by using a spectrophotometer, wherein the wavelength range is 380-780nm, and the reflectivity of the sample is tested.
5. Comparison of whiteness
And measuring the whiteness of the sample by using a whiteness meter.
6. Comparison of Exposure energies
And (3) exposing the sample by using an exposure machine, wherein the product does not wrinkle or yellow after thermal curing, and the exposure energy of the sample is tested.
7. Film coating property
Whether the surface of the coating film is flat or not and no particles exist.
The specific results of the cured film performance test are shown in table 1:
TABLE 1
| Bendability | Soldering heat resistance | Acid and alkali resistance | Reflectivity of light | Whiteness degree | Exposure energy | Film coating property | |
| Example 1 | ◎ | ◎ | ◎ | 91 | 94 | 250 | Leveling |
| Example 2 | ◎ | ◎ | ◎ | 92 | 94 | 150 | Leveling |
| Example 3 | ◎ | ◎ | ◎ | 90 | 94 | 300 | Leveling |
| Example 4 | ◎ | ◎ | ◎ | 90 | 94 | 100 | Leveling |
| Example 5 | ◎ | ◎ | ◎ | 93 | 94 | 200 | Leveling |
| Example 6 | ◎ | ◎ | ◎ | 95 | 94 | 500 | Leveling |
| Example 7 | ◎ | ◎ | ◎ | 90 | 94 | 500 | Leveling |
| Example 8 | ◎ | ◎ | ◎ | 90 | 94 | 200 | Leveling |
| Example 9 | ◎ | ◎ | ◎ | 90 | 94 | 500 | Leveling |
| Example 10 | ◎ | ◎ | ◎ | 90 | 94 | 100 | Leveling |
| Example 11 | ◎ | ◎ | ◎ | 90 | 94 | 200 | Leveling |
| Example 12 | ◎ | ◎ | ◎ | 92 | 94 | 200 | Leveling |
| Comparative example 1 | ◎ | ◎ | ◎ | 70 | 90 | 100 | Leveling |
| Comparative example 2 | ◎ | ◎ | ◎ | 90 | 94 | 500 | Unevenness of the skin |
| Comparative example 3 | ◎ | ◎ | ◎ | 50 | 50 | 100 | Leveling |
| Comparative example 4 | ◎ | ◎ | ◎ | 85 | 94 | 200 | Leveling |
Finally, comparing the above examples and comparative examples, the invention obtains the photosensitive covering film composition with uniform film thickness, less surface defects, better whiteness and reflectivity, good flexibility and high temperature resistance by selecting rutile type titanium dioxide and optimizing the dosage of each component. Particularly, compared with solder resist ink, the white photosensitive covering film provided by the invention adopts a single-component form, and can achieve the beneficial effects of good film forming property, high temperature resistance, flexibility, whiteness, light reflectivity and the like on the basis that the content of rutile titanium dioxide (the proportion of the rutile titanium dioxide relative to the alkali-soluble epoxy acrylic resin is less than or equal to 40%) is far lower than the content of the titanium dioxide in the solder resist ink.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (13)
1. The photosensitive covering film composition is characterized by comprising, by weight, 100 parts of alkali-soluble epoxy acrylic resin, 1-40 parts of epoxy resin, 1-40 parts of acrylate monomer, 0.1-10 parts of photoinitiator, 10-40 parts of rutile titanium dioxide and 0.5-2 parts of auxiliary agent.
2. The photosensitive coverlay composition according to claim 1, wherein the rutile titanium dioxide is 10 to 20 parts by weight; preferably, the rutile type titanium dioxide is one or more of R907, R900, R920, R931, R960, R102, R103, R104 and R105.
3. The photosensitive coverlay composition of claim 1, wherein the alkali soluble epoxy acrylic resin has an acid value of 60 to 150mg KOH/g, preferably 80 to 120mg KOH/g.
4. The photosensitive coverlay composition of any one of claims 1-3, wherein the alkali soluble epoxy acrylic resin is one or more of a carboxylic acid modified bisphenol A epoxy resin, a carboxylic acid modified bisphenol F epoxy resin, and a carboxylic acid modified novolac epoxy resin.
5. The photosensitive coverlay composition according to any one of claims 1 to 4, wherein the epoxy resin has an epoxy equivalent of 160 to 500g/eq and contains at least two epoxy groups; preferably, the epoxy resin is one or more of bisphenol epoxy resin, biphenyl epoxy resin, novolac epoxy resin, epoxy resin containing naphthalene ring and alicyclic epoxy resin; more preferably, the epoxy resin is the bisphenol type epoxy resin.
6. The photosensitive coverlay composition of claim 5, wherein the epoxy resin is 10 to 30 parts by weight.
7. The photosensitive coverlay composition of claim 4, wherein the acrylate monomer is one or more of monofunctional (meth) acrylate, difunctional (meth) acrylate, trifunctional (meth) acrylate, and multifunctional (meth) acrylate;
preferably, the monofunctional (meth) acrylate is one or more of (ethoxy) phenol (meth) acrylate, stearic acid acrylate, ethoxy (propoxy) nonylphenol (meth) acrylate, ethoxy (propoxy) tetrahydrofurfuryl (meth) acrylate;
preferably, the difunctional (meth) acrylate is one or more of 1, 6-hexanediol diacrylate, tricyclodecanedimethanol diacrylate, dioxane glycol diacrylate, ethoxylated (propoxylated) bisphenol a di (meth) acrylate, polyethylene glycol (400) diacrylate, polypropylene glycol (600) diacrylate;
preferably, the trifunctional (meth) acrylate is one or more of ethoxy (propoxy) trimethylolpropane tri (meth) acrylate, pentaerythritol triacrylate, tris (2-hydroxyethyl) isocyanurate triacrylate;
preferably, the multifunctional (meth) acrylate is one or more of dipentaerythritol hexaacrylate, ethoxylated pentaerythritol tetraacrylate, dipentaerythritol hexaacrylate.
8. The photosensitive coverlay composition of claim 7, wherein the weight average molecular weight of the acrylate monomer is 200-1000, and the glass transition temperature is-30-60 ℃; preferably, the weight part of the acrylate monomer is 5-30 parts.
9. The photosensitive coverlay composition of any one of claims 1-8, wherein the photoinitiator comprises a photopolymerization initiator and a photosensitizer, preferably in a weight ratio of (150-200): 1.
10. The photosensitive coverlay composition of claim 9, wherein the photopolymerization initiator is 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-1-propanone, 1- [4- (2-hydroxy) -phenyl ] -3-hydroxy-2-methyl-1-propanon-1-one, 2,4, 6-trimethylbenzoyl-diphenylphosphine oxide, bis (2,4, 6-trimethylbenzoyl) phenylphosphine oxide, ethyl 2,4, 6-trimethylbenzoylphenylphosphinate, 2-methyl-1- (4-methylthiophenyl) -2-morphinyl-1-propanone, methyl-1- (2-methyl-phenyl) -2-morphinyl-1-propanone, or mixtures thereof, One or more of 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-propanone;
preferably, the photosensitizer is one or more of 2, 4-diethyl oxalate, 2-isopropyl thioxanthone, 2, 4-diethyl thioxanthone and benzophenone.
11. The photosensitive coverlay composition of claim 9, wherein the photoinitiator is present in an amount of 1 to 5 parts by weight.
12. The photosensitive coverlay composition of any one of claims 1-11, wherein the auxiliary agent comprises one or more of a leveling agent, a defoaming agent, a dispersing agent, and an adhesion promoter; preferably, the leveling agent is one or more of BYK333, BYK358, BYK306, BYK394 and BYK322, the defoaming agent is one or more of BYK066N, BYK175, BYK015 and BYK1730, the dispersing agent is one or more of BKY110, BYK111 and BYK9077, and the adhesion promoter is BYK 4510.
13. The photosensitive coverlay composition of claim 12, wherein the auxiliary is 1-1.5 parts by weight.
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